ASTM C169-16(2022)
(Test Method)Standard Test Methods for Chemical Analysis of Soda-Lime and Borosilicate Glass
Standard Test Methods for Chemical Analysis of Soda-Lime and Borosilicate Glass
SIGNIFICANCE AND USE
3.1 These test methods can be used to ensure that the chemical composition of the glass meets the compositional specification required for the finished glass product.
3.2 These test methods do not preclude the use of other methods that yield results within permissible variations. In any case, the analyst should verify the procedure and technique employed by means of a National Institute of Standards and Technology (NIST) standard reference material having a component comparable with that of the material under test. A list of standard reference materials is given in the NIST Special Publication 260,3 current edition.
3.3 Typical examples of products manufactured using soda-lime silicate glass are containers, tableware, and flat glass.
3.4 Typical examples of products manufactured using borosilicate glass are bakeware, labware, and fiberglass.
3.5 Typical examples of products manufactured using fluoride opal glass are containers, tableware, and decorative glassware.
SCOPE
1.1 These test methods cover the quantitative chemical analysis of soda-lime and borosilicate glass compositions for both referee and routine analysis. This would be for the usual constituents present in glasses of the following types: (1) soda-lime silicate glass, (2) soda-lime fluoride opal glass, and (3) borosilicate glass. The following common oxides, when present in concentrations greater than indicated, are known to interfere with some of the determinations in this method: 2 % barium oxide (BaO), 0.2 % phosphorous pentoxide (P2O5), 0.05 % zinc oxide (ZnO), 0.05 % antimony oxide (Sb2O3), 0.05 % lead oxide (PbO).
1.2 The analytical procedures, divided into two general groups, those for referee analysis, and those for routine analysis, appear in the following order:
Sections
Procedures for Referee Analysis:
Silica
10
BaO, R2O2 (Al2O3 + P2O5), CaO, and MgO
11 – 15
Fe2O3, TiO2, ZrO2 by Photometry and Al2O3 by Com-
plexiometric Titration
16 – 22
Cr2O3 by Volumetric and Photometric Methods
23 – 25
MnO by the Periodate Oxidation Method
26 – 29
Na2O by the Zinc Uranyl Acetate Method and K2O by
the Tetraphenylborate Method
30 – 33
SO3 (Total Sulfur)
34 – 35
As2O3 by Volumetric Method
36 – 40
Procedures for Routine Analysis:
Silica by the Single Dehydration Method
42 – 44
Al2O3, CaO, and MgO by Complexiometric Titration,
and BaO, Na2O, and K2O by Gravimetric Method
45 – 51
BaO, Al2O3, CaO, and MgO by Atomic Absorption; and
Na2O and K2O by Flame Emission Spectroscopy
52 – 59
SO3 (Total Sulfur)
60
B2O3
61 – 62
Fluorine by Pyrohydrolysis Separation and Specific Ion
Electrode Measurement
63 – 66
P2O5 by the Molybdo-Vanadate Method
67 – 70
Colorimetric Determination of Ferrous Iron Using 1,10
Phenanthroline
71 – 76
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.4 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: C169 − 16 (Reapproved 2022)
Standard Test Methods for
Chemical Analysis of Soda-Lime and Borosilicate Glass
This standard is issued under the fixed designation C169; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.
1. Scope 1.3 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 These test methods cover the quantitative chemical
responsibility of the user of this standard to establish appro-
analysis of soda-lime and borosilicate glass compositions for
priate safety, health, and environmental practices and deter-
both referee and routine analysis. This would be for the usual
mine the applicability of regulatory limitations prior to use.
constituents present in glasses of the following types: (1)
1.4 This international standard was developed in accor-
soda-lime silicate glass, (2) soda-lime fluoride opal glass, and
dance with internationally recognized principles on standard-
(3) borosilicate glass. The following common oxides, when
ization established in the Decision on Principles for the
present in concentrations greater than indicated, are known to
Development of International Standards, Guides and Recom-
interfere with some of the determinations in this method: 2%
mendations issued by the World Trade Organization Technical
barium oxide (BaO), 0.2% phosphorous pentoxide (P O ),
2 5
Barriers to Trade (TBT) Committee.
0.05% zinc oxide (ZnO), 0.05% antimony oxide (Sb O ),
2 3
0.05% lead oxide (PbO).
2. Referenced Documents
1.2 The analytical procedures, divided into two general 2
2.1 ASTM Standards:
groups, those for referee analysis, and those for routine
C146Test Methods for Chemical Analysis of Glass Sand
analysis, appear in the following order:
C225Test Methods for Resistance of Glass Containers to
Sections
Chemical Attack
Procedures for Referee Analysis:
D1193Specification for Reagent Water
Silica 10
BaO, R O (Al O +P O ), CaO, and MgO 11–15 E50Practices for Apparatus, Reagents, and Safety Consid-
2 2 2 3 2 5
Fe O ,TiO ,ZrO by Photometry and Al O by Com- 16–22
2 3 2 2 2 3
erations for Chemical Analysis of Metals, Ores, and
plexiometric Titration
Related Materials
Cr O by Volumetric and Photometric Methods 23–25
2 3
MnO by the Periodate Oxidation Method 26–29 E60Practice for Analysis of Metals, Ores, and Related
Na O by the Zinc Uranyl Acetate Method and K Oby 30–33
2 2
Materials by Spectrophotometry
the Tetraphenylborate Method
SO (Total Sulfur) 34 – 35
3. Significance and Use
As O by Volumetric Method 36–40
2 3
3.1 These test methods can be used to ensure that the
Procedures for Routine Analysis:
chemical composition of the glass meets the compositional
Silica by the Single Dehydration Method 42–44
Al O , CaO, and MgO by Complexiometric Titration, 45–51
2 3 specification required for the finished glass product.
and BaO, Na O, and K O by Gravimetric Method
2 2
BaO, Al O , CaO, and MgO by Atomic Absorption; and 52–59
3.2 These test methods do not preclude the use of other
2 3
Na O and K O by Flame Emission Spectroscopy
2 2
methodsthatyieldresultswithinpermissiblevariations.Inany
SO (Total Sulfur) 60
case, the analyst should verify the procedure and technique
B O 61 – 62
2 3
Fluorine by Pyrohydrolysis Separation and Specific Ion 63–66 employed by means of a National Institute of Standards and
Electrode Measurement
Technology (NIST) standard reference material having a com-
P O by the Molybdo-Vanadate Method 67–70
2 5
ponentcomparablewiththatofthematerialundertest.Alistof
Colorimetric Determination of Ferrous Iron Using 1,10 71–76
Phenanthroline
standard reference materials is given in the NIST Special
Publication 260, current edition.
1 2
These test methods are under the jurisdiction of ASTM Committee C14 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Glass and Glass Products and are the direct responsibility of Subcommittee C14.02 contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
on Chemical Properties and Analysis. Standards volume information, refer to the standard’s Document Summary page on
CurrenteditionapprovedJuly1,2022.PublishedJuly2022.Originallyapproved the ASTM website.
in 1941. Last previous edition approved in 2016 as C169–16. DOI: 10.1520/ Available from National Institute of Standards and Technology, Gaithersburg,
C0169-16R22. MD 20899.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
C169 − 16 (2022)
3.3 Typical examples of products manufactured using soda- “Medium” filter paper refers to that used for filtration of
lime silicate glass are containers, tableware, and flat glass. calcium oxalate, and “fine” filter paper to that used for barium
sulfate.
3.4 Typical examples of products manufactured using boro-
silicate glass are bakeware, labware, and fiberglass.
7. Photometers and Photometric Practice
3.5 Typical examples of products manufactured using fluo-
7.1 Photometers and photometric practice prescribed in
ride opal glass are containers, tableware, and decorative
these methods shall conform to Practice E60.
glassware.
7.2 The considerations of instrumentation given in Test
4. Purity of Reagents Methods C146 are equally applicable to these test methods.
4.1 Reagent grade chemicals shall be used throughout.
8. Preparation of Sample
Unless otherwise indicated, it is intended that reagents shall
8.1 Glass crushed in a steel mortar as described in Test
conform to the specifications of the Committee on Analytical
Methods C225, and sieved through a 150µm (No. 100) mesh
Reagents of the American Chemical Society, where such
sieve, is generally suitable for analysis, except for the deter-
specifications are available. Other grades may be used, pro-
mination of iron oxide (Fe O ). After crushing and sieving,
vided it is first ascertained that the reagent is of sufficiently
2 3
place the powder on a sheet of paper and pass a small magnet
high purity to permit its use without lessening the accuracy of
through it to remove adventitious iron. Then store in a tightly
the determination.
closed container and keep in a desiccator.
4.2 Purity of Water—Unless otherwise indicated, reference
8.2 A sample prepared in an iron mortar is not recom-
to water shall be understood to mean reagent water as defined
mended for the determination of Fe O . Instead, glass should
by Type I, II, or III of Specification D1193.
2 3
be ground in an agate mortar after ascertaining it is free of
contamination.
5. Concentration of Acids and Ammonium Hydroxide
5.1 When acids and ammonium hydroxide are specified by 8.3 A sample prepared for the determination of fluorine
should be sieved through a 75µm (No. 200) mesh sieve rather
name or chemical formula only, concentrated reagents of the
following percent concentrations are intended: than a 150µm (No. 100) sieve.
%
8.4 The practice of drying samples in a drying oven at
Hydrochloric acid (HCl) 36 to 38
105°C to 110°C after preparation is not recommended.
Hydrofluoric acid (HF) 48 to 51
Powdered glass can fix CO and water as readily at this
Nitric acid (HNO ) 69to71
Perchloric acid (HClO ) 70to72
temperatureasatroomtemperature.Afreshlypreparedsample,
Sulfuric acid (H SO ) 95to98
2 4
if exposed but a short time to the atmosphere, will not have
Ammonium hydroxide (NH OH) 28 to 30
acquired an ignition loss of much analytical significance. If
ignition loss is determined, use the following temperature
5.2 Concentrations of diluted acids and NH OH except
schedules:
when standardized are specified as a ratio, stating the number
of volumes of the concentrated reagent to be added to a given
Soda-lime glass 800 °C for 1 h
number of volumes of water, as follows: HCl (1 + 99) means
Fluorine opal glass 500 °C to 550 °C for 1 h
1 volume of concentrated HCl (approximately 37%) added to
Borosilicate glass 800 °C for 1 h
99 volumes of water.
Determine the ignition loss on a 1g to 3g sample in a
5.3 The hygroscopic nature of the ignited precipitates of
platinum crucible.
silica, aluminum oxide, and calcium oxide obtained in the
methods to be described, requires the use of fresh and highly
9. Precision and Bias
active desiccants. For this purpose, magnesium perchlorate
9.1 The probable precision of results that can be expected
(Mg(ClO ) ) and barium oxide (BaO) are recommended.
4 2
by the use of the procedures described in these test methods is
6. Filter Papers shown in the following tabulation. Precision is given as
absolute error, and is dependent on the quantity of constituent
6.1 Throughout these test methods, filter papers will be
present as well as the procedure used.
designated as “coarse,” “medium,” or “fine,” without naming
Probable Precision of Results, weight %
brandsormanufacturers.Allfilterpapersareofthedoubleacid
washedashlesstype.“Coarse”filterpaperreferstotheporosity
Constituent Referee Analysis Routine Analysis
commonly used for the filtration of aluminum hydroxide.
Silica ±0.1 ±0.25
BaO ±0.02 ±0.05
Al O +P O ±0.05 ±0.10 (−P O )
2 3 2 5 2 5
CaO ±0.05 ±0.15
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
MgO ±0.05 ±0.02 to 0.10
Standard-Grade Reference Materials, American Chemical Society, Washington,
Fe O ±0.003 . . .
DC. For suggestions on the testing of reagents not listed by theAmerican Chemical 2 3
TiO ±0.005 . . .
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset,
ZrO ±0.001 to 0.005 . . .
U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
Cr O (volumetric) ±0.005 . . .
2 3
copeial Convention, Inc. (USPC), Rockville, MD.
C169 − 16 (2022)
Cr O (photometric) ±0.0001 to 0.001 . . . Percent Number of Significant Figures
2 3
MnO ±0.001 to 0.005 . . . Retained After Rounding
Na O ±0.05 ±0.25 (flame emission) 1to100 3
K O ±0.02 to 0.05 ±0.02 to 0.10 (flame emission) 0.1to0.99 2
SO ±0.02 ±0.05 0.01 to 0.09 1 or 2
As O ±0.005 . . . <0.01 1 or 2
2 3
P O . . . ±0.005 to 0.02
2 5
9.3 Recorded results should be carried to one more signifi-
B O . . . ±0.05 to 0.15
2 3
Fluorine . . . ±0.01 to 0.20 (0.1 to 6.0 %)
cant figure than required in 9.2.
9.2 It is recommended that reported results be rounded as
follows:
PROCEDURES FOR REFEREE ANALYSIS
SILICA stirring rod and the periphery of the funnel with a piece of
damp filter paper and add to the dish containing the precipitate
for ignition.
10. Procedure
10.1 Weigh 1.000 g of powdered sample and 1.5 g of NOTE 1—Glasses containing fluorine in small amounts (less than
0.25%)willnotcausesignificanterror.Glassescontaininglargeramounts
anhydrous sodium carbonate (Na CO ) for soda-lime glass, or
2 3
of fluorine (for example, fluoride opals) are analyzed as above with this
2.0g of Na CO for borosilicate glass, into a clean 75mL
2 3
exception: after the fusion has been made and before addition of the acid
platinum dish (see 10.1.1); mix well with a platinum or
(see 10.2), add 10 mL of aluminum chloride (AlCl ) solution
Nichrome wire. Tap the charge so it lies evenly in the bottom
(10mL=200 mg ofAl) to complex fluorine. If evaporation is made on a
steambath,itisdifficulttodrytheresidue.Itissuggestedthatfinaldrying,
of the dish. Cover with platinum lid and heat first at a dull red
before filtration, be made in a drying oven for 30 to 45 min at 105°C.
heat over a clean oxidizing flame; gradually raise the tempera-
Results for SiO when analyzing fluorine opals may tend to be low by
ture until a clear melt is obtained. Properly carried out, little or
0.2% to 0.3%. For an alternative, but more lengthy procedure, consult
no spattering should occur and the fusion can be performed in
Applied Inorganic Analysis.
3 to 4 min. When melted, rotate the melt to spread it evenly
NOTE 2—Boron in amounts less than 5% B O does not interfere.
2 3
However, if boron is greater than 5%, proceed to the point of completing
over the bottom and lower sides of the dish, gradually
the first dehydration (see 10.2), then add 20 mL of anhydrous methanol
withdrawing from the flame. Cover and cool to room tempera-
saturated with dry HCl (gas), and evaporate to dryness on an air bath or
ture.Duringfusion,thedishshouldbehandledatalltimeswith
under an infrared lamp. Repeat once more before proceeding.
platinum-tipped tongs and the fusion performed with a plati-
10.3 Evaporate the filtrate to dryness on the steam bath or
num (preferably 90% platinum and 10% rhodium alloy) or
under an infrared lamp.When dry, cool, drench with 10 mLof
silica triangle.
HCl (1+1) and again evaporate just to dryness; then bake in a
10.1.1 To obtain accurate repeat weighings, platinum ware
drying oven at 105°C for 30 min. Cool, drench with 5 mL of
shall be kept scrupulously clean on the outside of the vessel as
HCl, and add 20 mLof hot water and a small bit of filter pulp.
well as on the inside. It should be polished brightly with fine,
Digesthotfor5minandfilterthrougha7cmfinepaper.Police
round grain sand and protected from dirty surfaces. It is
thedishwiththeaidofabitofpaperpulpandwashprecipitate
recommendedthatporcelainplatesbeusedforcoolingfusions,
andpapereighttimeswithhot2%HCl.Transferthepaperand
andthatplatinumbesetonpapertowelsorothercleanmaterial
precipitate to the dish containing the initial precipitation.Wipe
during filtration.
the stirring rod and the periphery of the funnel with a piece of
10.2 Add 20mL to 25 mL of HCl (1 + 1) (Note 1) under
damp filter paper and add to the dish containing the precipitate
theplatinumcoveranddigestonasteambathorhotplateuntil
for ignition.
the melt has completely disintegrated; it is also possible to
10.4 Partially cover the dish with its platinum lid but leave
digest the melt in the cold overnight. Police and rinse the lid
enoughspacesoaircancirculateduringignition.Placethedish
with a fine jet of water; rinse down the sides of the dish and
in a cold muffle furnace and bring the temperature to 1200°C
evaporatetodrynessonasteambathorunderaninfraredlamp.
for 30 min. Carefully and completely cover the dish before
Keep the dish covered with a raised cover glass during
removing it from the furnace and transfer to a desiccator. Cool
evaporation. When evaporation is complete (Note 2) (absence
toroomtemperatureandweighthecovereddish(W ).Moisten
of HCl), cool, drenc
...
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